CN102543270B - Grapheme-based composite film and preparation method therefor, conductive electrode and preparation method therefor - Google Patents
Grapheme-based composite film and preparation method therefor, conductive electrode and preparation method therefor Download PDFInfo
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- CN102543270B CN102543270B CN201210021877.XA CN201210021877A CN102543270B CN 102543270 B CN102543270 B CN 102543270B CN 201210021877 A CN201210021877 A CN 201210021877A CN 102543270 B CN102543270 B CN 102543270B
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Abstract
The embodiment of the invention discloses a grapheme-based composite film which comprises a grapheme thin film layer and a silk fibroin thin film layer, wherein the grapheme thin film layer is in solidification combination with the surface of the silk fibroin thin film layer. The invention further discloses a grapheme-based composite film preparation method, a conductive electrode and a preparation method therefor. The grapheme-based composite film provided by the invention combines the superior photoelectric property of the grapheme and the excellent light transmission performance of the silk fibroin thin film and has the advantages of favorable photoelectric property, light transmission performance, thermal conduction performance, good flexibility, thin thickness, and the like. The prepared composite thin film has the advantages of simple technology, abundant raw material resource and low cost; and the silk fibroin substrate and the grapheme conductive filling material are separately processed, and the damage to the silk fibroin substrate is small.
Description
Technical field
The invention belongs to grapheme material technical field, more particularly, relate to a kind of composite membrane based on Graphene and preparation method thereof, conductive electrode and preparation method thereof.
Background technology
At present, ITO (Indium-Tin Oxide), as transparent conductive material main on market, is widely used at emerging fields such as thin-film solar cells.ITO has and is greater than 90% light transmittance, sheet resistance to reach that 10-30 Ω/square centimeter, electronics overflow can be～4.8eV.But the deficiency of indium resource, complicated preparation technology, to environment, particularly sour environment sensitivity, rough surface etc. make the use of ITO have limitation; In addition, ITO is flexible poor, frangible, and very easy fracture when being applied in touch-screen, flexible display etc. and having in crooked condition, has a strong impact on its performance.
Graphene (Graphene), claims again mono-layer graphite, is a kind ofly by carbon atom, with sp2 hybridized orbit, to form the flat film that hexangle type is honeycomb lattice, only has the two-dimensional material of a carbon atom thickness.The charming part of Graphene is not only the two-dimensional structure of its mystery, is also unique physical property that it has.Since Graphene is found, caused a large amount of scientific workers' concern.So far, found the many peculiar character that Graphene all has at aspects such as electricity, light and magnetic.Graphene be at present the thinnest be in the world the hardest nano material also, it is almost completely transparent, only absorbs 2.3% light; Conductive coefficient is up to 5300W/mK, and higher than carbon nano-tube and diamond, under normal temperature, its electron mobility surpasses 15000cm2/Vs, ratio nano carbon pipe or silicon wafer height again, and resistivity about 10-6 Ω cm is only lower than copper or silver, it is the material of resistivity minimum in the world at present.The good chemistry of Graphene and thermal stability, excellent tensile property, low contact resistance are combined with organic material, make Graphene application as transparency electrode in organic electronic device there is very large advantage and good prospect, such as: organic light emitting diode, LCDs, touch-screen, field effect transistor etc.
Fibroin has excellent film-forming quality, fibroin rete has excellent light transmission and pliability, and its good biocompatibility, the mechanical performance of excellence and controlled biodegradability, be widely used in every field in addition.The rich aboundresources of fibroin, has been established solid foundation for being widely used in from now on photoelectric field.
Summary of the invention
For the deficiencies in the prior art, the technical problem that the present invention solves is to provide a kind of composite membrane based on Graphene and preparation method thereof, conductive electrode and preparation method thereof, and the composite membrane thin thickness obtaining, flexible, cost is low and have good photoelectric properties, light transmission and heat conductivility.
For solving the problems of the technologies described above, technical scheme of the present invention is achieved in that a kind of composite membrane based on Graphene, especially, described composite membrane comprises graphene film layer and silk protein films layer, and described graphene film layer solidifies the surface that is incorporated into described silk protein films layer.
Correspondingly, the present invention also provides a kind of preparation method of the composite membrane based on Graphene, especially, comprises the steps:
(1) prepare graphene film;
(2) prepare silk protein films;
(3) graphite fine film and silk protein films are compound, obtain the composite membrane based on Graphene.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, the preparation method of described step (1) is implemented as follows:
(a) graphene oxide solution is coated on silicon chip, obtains graphene oxide film;
(b) graphene oxide film is immersed in hydroiodic acid solution and is reduced, obtain graphene film.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, in described step (a), described graphene oxide solution is coated on silicon chip by rotary coating method.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, the concentration of described graphene oxide solution is 1.5mg/ml, and the rotating speed of described rotary coating is 3000 revs/min.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, the preparation method of described step (2) is implemented as follows:
One, prepare silk fibroin protein solution;
Two, silk fibroin protein solution is applied in to the surface of graphene film, the dry rear silk protein films that is formed at Graphene surface that obtains.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, the preparation of described graphene film is carried out on silicon chip, after prepared by silk protein films, graphene film and silk protein films are peeled off from silicon chip, obtained the composite membrane based on Graphene.
The present invention also provides a kind of preparation method of conductive electrode, especially, the above-mentioned composite membrane based on Graphene is carried out to photoetching treatment, obtains conductive electrode.
Correspondingly, the present invention also provides a kind of conductive electrode, and especially, described conductive electrode is to adopt above-mentioned method to obtain.
From above-mentioned technical scheme, can find out, the invention provides a kind of composite membrane based on Graphene, it combines the light transmission of the good photoelectric properties of Graphene and silk protein films excellence, not only there is good photoelectric properties, light transmission and heat conductivility, also there is the advantages such as degree of flexibility is good, thin thickness.Meanwhile, the prepared laminated film technique of the present invention is simple, raw material resources abundant, cost is low, and silk-fibroin substrate and graphene conductive packing material separate machined are little to the infringement of silk-fibroin substrate.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, to the accompanying drawing of required use in embodiment be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 the present invention is based on the composite membrane preparation method's of Graphene block diagram.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the invention discloses a kind of composite membrane based on Graphene, wherein, described composite membrane comprises graphene film layer and silk protein films layer, and described graphene film layer solidifies the surface that is incorporated into described silk protein films layer.
Fibroin not only has excellent film-forming quality and excellent light transmission, but also has good biocompatibility, the mechanical performance of excellence and controlled biodegradability.The compound acquisition composite membrane of fibroin and Graphene, has not only retained the good characteristic of Graphene, also has good flexibility and good light transmission, due to fibroin film can do very thin, can reduce the thickness of silk protein films substrate.Meanwhile, because fibroin raw material resources are abundant, price is low, it is easy to obtain, can reduce the cost of composite membrane.
Shown in ginseng Fig. 1, correspondingly, the embodiment of the invention discloses a kind of preparation method of the composite membrane based on Graphene, wherein, comprise the steps:
(1) prepare graphene film;
(2) prepare silk protein films;
(3) graphite fine film and silk protein films are compound, obtain the composite membrane based on Graphene.
Above-mentioned preparation method is simple, can produce in a large number, and due to silk protein films and graphene film separate machined, little to the infringement of silk-fibroin substrate.
In above-mentioned preparation method, can first prepare graphene film, then on graphene film, apply silk fibroin protein solution, then by the dry silk protein films that obtains; In above-mentioned preparation method, can also realize like this: first prepare silk protein films, and then on silk protein films, prepare graphene film.
Preferably, the preparation method of described step (1) is implemented as follows:
(a) graphene oxide solution is coated on silicon chip, obtains graphene oxide film;
(b) graphene oxide film is immersed in hydroiodic acid solution and is reduced, obtain graphene film.
In described step (a), described graphene oxide solution is coated on silicon chip by rotary coating method.The concentration of described graphene oxide solution is preferably 1.5mg/ml, and the rotating speed of described rotary coating is preferably 3000 revs/min.Described graphene oxide solution can also be coated on silicon chip by other means of the prior art, such as modes such as sprayings, in the present invention, does not limit.
The preparation method of graphene film is also not limited to above-mentioned means, can also obtain by methods such as chemical vapour deposition techniques.
Preferably, the preparation method of described step (2) is implemented as follows:
One, prepare silk fibroin protein solution;
Two, silk fibroin protein solution is applied in to the surface of graphene film, the dry rear silk protein films that is formed at Graphene surface that obtains.
Preferably, in the preparation method of the above-mentioned composite membrane based on Graphene, the preparation of described graphene film is carried out on silicon chip, after prepared by silk protein films, graphene film and silk protein films are peeled off from silicon chip, obtained the composite membrane based on Graphene.
By peeling off means, the composite membrane based on Graphene is taken off from silicon chip, simple to operate, little to the composite membrane destructiveness based on Graphene.
The embodiment of the present invention also provides a kind of preparation method of conductive electrode, wherein, the above-mentioned composite membrane based on Graphene is carried out to photoetching treatment, obtains conductive electrode.
The embodiment of the present invention also provides a kind of conductive electrode, and wherein, described conductive electrode is to adopt above-mentioned preparation method to obtain.
Due to the superperformance of composite membrane, prepared conductive electrode also has good flexibility and light transmission thus.
In order to further illustrate technical scheme of the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The preparation method of Graphene/silk-fibroin composite membrane and conductive electrode is as follows:
(1) use the graphene oxide solution (ethanol: water=2: 1) spin coating one deck graphene oxide film (rotating speed: 3000 revs/min) on silicon chip of 1.5mg/ml;
(2) the good graphene oxide film of spin coating is immersed in hydroiodic acid solution and is reduced, obtain graphene film;
(3) by conventional means, prepare silk fibroin protein solution;
(4) on graphene film surface, drip a certain amount of silk fibroin protein solution, air-dry after, on graphene film surface, form silk protein films, thereby obtain Graphene/silk-fibroin composite membrane;
(5) Graphene/fibroin laminated film is peeled off from silicon chip surface;
(6) Graphene/fibroin laminated film is carried out to photoetching treatment, obtain conductive electrode.
In sum, the invention has the advantages that: the composite membrane based on Graphene provided by the invention, it combines the light transmission of the good photoelectric properties of Graphene and silk protein films excellence, not only there is good photoelectric properties, light transmission and heat conductivility, also there is the advantages such as mechanical performance that degree of flexibility is good, good and thin thickness.Meanwhile, the prepared laminated film technique of the present invention is simple, raw material resources abundant, cost is low, and silk-fibroin substrate and graphene conductive packing material separate machined are little to the infringement of silk-fibroin substrate.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other concrete form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, is therefore intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in scope.Any Reference numeral in claim should be considered as limiting related claim.
In addition, be to be understood that, although this specification is described according to execution mode, but not each execution mode only comprises an independently technical scheme, this narrating mode of specification is only for clarity sake, those skilled in the art should make specification as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other execution modes that it will be appreciated by those skilled in the art that.
Claims (9)
1. the composite membrane based on Graphene, is characterized in that, described composite membrane comprises graphene film layer and silk protein films layer, and described silk protein films layer solidifies the surface that is incorporated into described graphene film layer.
2. a preparation method for the composite membrane based on Graphene as claimed in claim 1, is characterized in that, comprises the steps:
(1) prepare graphene film;
(2) prepare silk protein films;
(3) graphite fine film and silk protein films are compound, obtain the composite membrane based on Graphene.
3. the preparation method of the composite membrane based on Graphene according to claim 2, is characterized in that, the preparation method of described step (1) is implemented as follows:
(a) graphene oxide solution is coated on silicon chip, obtains graphene oxide film;
(b) graphene oxide film is immersed in hydroiodic acid solution and is reduced, obtain graphene film.
4. the preparation method of the composite membrane based on Graphene according to claim 3, is characterized in that, in described step (a), described graphene oxide solution is coated on silicon chip by rotary coating method.
5. the preparation method of the composite membrane based on Graphene according to claim 4, is characterized in that, the concentration of described graphene oxide solution is 1.5mg/ml, and the rotating speed of described rotary coating is 3000 revs/min.
6. the preparation method of the composite membrane based on Graphene according to claim 2, is characterized in that, the preparation method of described step (2) is implemented as follows:
One, prepare silk fibroin protein solution;
Two, silk fibroin protein solution is applied in to the surface of graphene film, the dry rear silk protein films that is formed at Graphene surface that obtains.
7. the preparation method of the composite membrane based on Graphene according to claim 6, it is characterized in that, the preparation of described graphene film is carried out on silicon chip, after prepared by silk protein films, graphene film and silk protein films are peeled off from silicon chip, obtained the composite membrane based on Graphene.
8. a preparation method for conductive electrode, is characterized in that, the described composite membrane based on Graphene claimed in claim 1 is carried out to photoetching treatment, obtains conductive electrode.
9. a conductive electrode, is characterized in that, described conductive electrode is to adopt method claimed in claim 8 to obtain.
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| CN102940907A (en) * | 2012-11-09 | 2013-02-27 | 南京工业大学 | Graphene oxide and silk fibroin composite membrane and preparation method thereof |
| CN103236324A (en) * | 2013-04-22 | 2013-08-07 | 南京邮电大学 | Method for preparing reduced graphene oxide-based flexible transparent conductive thin film |
| KR101473312B1 (en) * | 2013-05-31 | 2014-12-16 | 삼성디스플레이 주식회사 | A touch screen panel and a flexible display apparatus including the same |
| CN103611192B (en) * | 2013-11-13 | 2015-03-18 | 江苏科技大学 | Partially reduced graphene oxide-silk fibroin composite film, and preparation method and application thereof |
| CN103572395B (en) * | 2013-11-14 | 2015-08-12 | 东华大学 | A kind of activeness and quietness regenerated silk fiber and preparation method thereof |
| CN103762014A (en) * | 2013-12-24 | 2014-04-30 | 苏州大学 | Flexible and transparent electrode film based on silk fibroin and manufacturing method and application thereof |
| CN103871548B (en) * | 2014-02-28 | 2016-08-31 | 南京邮电大学 | A kind of flexible transparent film electrode and preparation method thereof |
| CN104986759B (en) * | 2015-07-03 | 2017-06-09 | 苏州大学 | Graphene/porous ferric oxide nanometer rods compound and preparation method thereof |
| CN106183508B (en) * | 2016-07-19 | 2018-11-02 | 南通纺织丝绸产业技术研究院 | Optical anti-counterfeiting label based on fibroin and preparation method thereof |
| CN107121471A (en) * | 2017-06-27 | 2017-09-01 | 苏州奥特科然医疗科技有限公司 | A kind of ELIASA |
| CN107610816B (en) * | 2017-09-17 | 2019-08-02 | 江苏华佳丝绸股份有限公司 | Based on silver nanowires/graphene silk base flexible transparent conductive film |
| CN112126096B (en) * | 2020-08-24 | 2022-04-26 | 江苏大学 | Silk fibroin uniformly-supported graphene composite membrane, preparation method and application thereof |
| CN115678092A (en) * | 2022-04-24 | 2023-02-03 | 复向丝泰医疗科技(苏州)有限公司 | Silk protein flexible electrode capable of monitoring muscle nerve injury and preparation method thereof |
| CN115655502B (en) * | 2022-12-29 | 2023-03-17 | 中北大学 | Temperature sensor based on piezoresistive characteristic of suspended graphene film |
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Inventor after: Zhang Keqin Inventor after: Liu Zhuang Inventor after: Qi Ning Inventor after: Jia Mingliang Inventor after: Zhang Shuai Inventor before: Zhang Keqin Inventor before: Liu Zhuang Inventor before: Jia Mingliang Inventor before: Zhang Shuai |
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